反应详情

温度

60 °C

24.59 g (132.8 mmol) of potassium phthalimide are added to a solution of 14.3 ml (124.4 mmol) of 5-chloro-2-pentanone in 100 ml of DMF and the mixture is left to stir at room temperature for 3 h and at 60° C. for 30 h. After filtering, the filtrate is partitioned between water and dichloromethane. The phases are separated and the organic phase is washed successively with water, twice with an 0.2N solution of NaOH and water and then dried over sodium sulfate. After filtering, the solvent is removed in vacuo and the residue is chromatographed through silica gel using heptane/ethyl acetate=6/4. 9.8 g (34%) of (14.1) are obtained after concentrating the product fractions.

1. waitthe mixture is left
2. filtrationAfter filtering
3. customthe filtrate is partitioned between water and dichloromethane
4. customThe phases are separated
5. washthe organic phase is washed successively with water, twice with an 0.2N solution of NaOH and water
6. dry with materialdried over sodium sulfate
7. filtrationAfter filtering
8. customthe solvent is removed in vacuo
9. customthe residue is chromatographed through silica gel